摘要
目的建立高效液相色谱波长切换法测定黄连上清丸中12种成分含量的方法。方法采用Welch-Ultimate-C_(18)色谱柱(4.6 mm×250 mm,5μm);以乙腈-0.3%磷酸溶液为流动相;柱温30℃;流速1 m L·min^(-1);切换波长检测。结果在HPLC法中,黄柏碱、甘草苷、黄芩苷、小檗碱、黄芩素、芦荟大黄素、大黄酸、欧前胡素、大黄素、异欧前胡素、大黄酚、大黄素甲醚的线性范围分别是:248~1736 ng(r=0.9996)、82.94~580.58 ng(r=1.0000)、68.54~685.4 ng(r=0.9999)、33.8~236.6 ng(r=0.9996)、149.6~1047.2 ng(r=0.9999)、31.54~220.78 ng(r=1.0000)、27.74~267.4 ng(r=0.9998)、7.68~53.76 ng(r=0.9999)、32.84~229.88 ng(r=0.9998)、4.26~29.82 ng(r=0.9999)、49.26~492.6 ng(r=0.9999)、9.86~98.6 ng(r=1.0000);平均回收率及RSD均符合药典规定。结论所建方法专属性强,重复性好,可用黄连上清片的质量控制。
Objective To establish a method to simultaneously determine 12 compounds in Huanglian Shangqing pills by HPLC combined with wavelength switching method. Methods The chromatograhic column was Welch-Ultimate-C_(18)(4.6 mm×250 mm, 5 μm); the column temperature was maintained at 30 ℃; A linear elution of 0.3% phosphoric acid aqueous solution acetonitrile was adopted at 1 m L·min(-1). The. UV detection wavelength was switched. Results Phellodendrine, lliquiritin, baicalin, berberine, baicalein, aloeemodin, rhein, imperatorin, emodin, isoimperatorin, chrysophanol, and physcion had good linearity at 248- 1736 ng(r =0.9996), 82.94- 580.58 ng(r = 1.0000), 68.54- 685.4 ng(r = 0.9999), 33.8- 236.6 ng(r = 0.9996), 149.6- 1047.2 ng(r = 0.9999), 31.54- 220.78 ng(r = 1.0000), 27.74- 267.4 ng(r = 0.9998), 7.68-53.76 ng(r = 0.9999), 32.84- 229.88 ng(r = 0.9998), 4.26- 29.82 ng(r = 0.9999), 49.26- 492.6 ng(r= 0.9999) and 9.86- 98.6 ng(r = 1.0000), respectively. The average recoveries all meet the requirements of Pharmacopoeia. Conclusion This method is simple accurate and reproduceable, which can be used for the quality control of Huanglian Shangqing pill.
出处
《中南药学》
CAS
2016年第8期851-854,共4页
Central South Pharmacy